Synthesis and crystal structure of NaCuIn(PO4)2

Benhsina, E.; Khmiyas, J.; Ouaatta, S.; Assani, A.; Saadi, M.; El Ammari, L.

doi:10.1107/S2056989020001929

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Volume 76| Part 3| March 2020| Pages 366-369

https://doi.org/10.1107/S2056989020001929

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Synthesis and crystal structure of NaCuIn(PO₄)₂

Elhassan Benhsina,^a ^* Jamal Khmiyas,^a Said Ouaatta,^a Abderrazzak Assani,^b Mohamed Saadi ^b and Lahcen El Ammari ^b

^aLaboratoire de Chimie Appliquée des Matériaux, Centre des Sciences des Matériaux, Faculty of Sciences, Mohammed V University in Rabat, Avenue Ibn Batouta, BP 1014, Rabat, Morocco, and ^bLaboratoire de Chimie Appliquée des Matériaux, Centre des Sciences des Matériaux, Faculty of Sciences, Mohammed V University in Rabat, Avenue Ibn Batouta, B.P. 1014, Rabat, Morocco
^*Correspondence e-mail: el_benhsina@yahoo.fr

Edited by M. Weil, Vienna University of Technology, Austria (Received 20 January 2020; accepted 10 February 2020; online 14 February 2020)

Single crystals of sodium copper(II) indium bis[phosphate(V)], NaCuIn(PO₄)₂, were grown from the melt under atmospheric conditions. The title phosphate crystallizes in the space group P2₁/n and is isotypic with KCuFe(PO₄)₂. In the crystal, two [CuO₅] trigonal bipyramids share an edge to form a dimer [Cu₂O₈] that is connected to two PO₄ tetrahedra. The obtained [Cu₂P₂O₁₂] units are interconnected through vertices to form sheets that are sandwiched between undulating layers resulting from the junction of PO₄ tetrahedra and [InO₆] octahedra. The two types of layers are alternately stacked along [101] and are joined into a three-dimensional framework through vertex- and edge-sharing, leaving channels parallel to the stacking direction. The channels host the sodium cations that are surrounded by four oxygen atoms in form of a distorted disphenoid.

Keywords: crystal structure; phosphate; AMM'(PO₄)₂ family; trigonal–bipyramidal coordination; isotypism.

CCDC reference: 1983244

1. Chemical context

Transition-metal phosphates have been the subject of intensive research as a result of their interesting physical properties and potential applications in wide-ranging fields such as catalysis, electrochemistry, luminescence (Tie et al., 1995 ; Pan et al., 2006 ; Yang et al., 2016 ) and ion exchange (Cheetham et al., 1999 ; Han et al., 2015 ; Manos et al., 2005 , 2007 ; Plabst et al., 2009 ; Stadie et al., 2017 ). In these materials, the anionic framework is built up from PO₄ tetrahedra linked to different kinds of transition metal (TM) coordination polyhedra of the form [TMO_n] (n = 4, 5 and 6), leading to a large variety of crystal structure families. This structural diversity is mainly associated with the ability of TM cations to adopt different oxidation states in various coordination polyhedra. Based on previous hydrothermal investigations aimed at orthophosphates of general formula (M,M′′)₃(PO₄)₂·nH₂O (M and M′′ = bivalent cations), we have reported on synthesis and characterization of the phosphates Ni₂Sr(PO₄)₂·2H₂O (Assani et al., 2010 ), Mg_1.65Cu_1.35(PO₄)₂·H₂O (Khmiyas et al., 2015 ) and Mn₂Zn(PO₄)₂·H₂O (Alhakmi et al., 2015 ). In this context, the aim of the present study was to develop new phases belonging to the series AM′′M′′′(PO₄)₂ where A, M′′ and M′′′ are mono-, bi- and trivalent cations, respectively. As a result, we report here on synthesis and crystal structure of the new compound NaCuIn(PO₄)₂.

2. Structural commentary

The principal building units of the crystal structure of NaCuIn(PO₄)₂ are two PO₄ tetrahedra linked to a [CuO₅] triangular bipyramid [Cu—O bond-length range of 1.9088 (9) to 2.1939 (9) Å] and to an [InO₆] octahedron [In—O bond lengths range from 2.1028 (10) to 2.2051 (9) Å], and is completed by a distorted [NaO₄] polyhedron (Fig. 1). The P—O bond lengths in the two phosphate tetrahedra are similar and comparable with those of similar phosphates. However, the P1—O distances, varying between 1.5035 (10) and 1.5729 (9) Å, indicate a somewhat higher distortion of this tetrahedron than the P2—O distances [between 1.5297 (9) and 1.5488 (9) Å] of the other tetrahedron.

Figure 1
The principal building units in the crystal structure of NaCuIn(PO₄)₂. Displacement ellipsoids are drawn at the 50% probability level. [Symmetry codes: (i) x + $[{1\over 2}]$ , −y − $[{1\over 2}]$ , z + $[{1\over 2}]$ ; (ii) −x + 1, −y, −z + 2; (iii) −x + $[{1\over 2}]$ , y − $[{1\over 2}]$ , −z + $[{3\over 2}]$ ; (iv) x + $[{1\over 2}]$ , −y + $[{1\over 2}]$ , z + $[{1\over 2}]$ ; (v) −x + 1, −y, −z + 1; (vi) x, y, z + 1; (vii) −x, −y, −z + 1; (viii) −x + $[{1\over 2}]$ , y + $[{1\over 2}]$ , −z + $[{3\over 2}]$ ; (ix) x − $[{1\over 2}]$ , −y + $[{1\over 2}]$ , z + $[{1\over 2}]$ .]

In this phosphate, two [CuO₅] triangular bipyramids share one edge to form a [Cu₂O₈] dimer, the ends of which are linked to two P1O₄ tetrahedra by edge-sharing. The obtained [Cu₂P₂O₁₂] groups are linked together via the vertices to form sheets extending parallel to (10 $[\overline{1}]$ ), as shown in Fig. 2. On the other hand, the [InO₆] octahedra and the P2O₄ tetrahedra are interconnected through common vertices to build up an undulating layer extending in the same direction (Fig. 3). The copper phosphate layers are sandwiched between the undulating indium phosphate layers. By sharing corners and edges, an alternating stacking of the layers along [101] leads to a three-dimensional framework structure with channels in which the Na⁺ cations are located (Fig. 4). The four nearest oxygen atoms around the alkali metal cation form a distorted disphenoid with Na—O distances between 2.3213 (12) and 2.4275 (11) Å (Fig. 1).

Figure 2
Projection along [001] of [Cu₂P₂O₁₂] copper phosphate sheets in the crystal structure of NaCuIn(PO₄)₂.

Figure 3
(a) A view approximately along [101] showing the undulating layer formed by [InO₆] octahedra linked to PO₄ tetrahedra and (b) a projection of this layer onto (101).

Figure 4
The sodium cations located in channels running parallel to [101] in the crystal structure of NaCuIn(PO₄)₂.

NaCuIn(PO₄)₂ is isotypic with KCuFe(PO₄)₂ (Badri et al., 2011 ), whereby potassium is substituted by sodium and iron by indium. However, we note a significant difference in the coordination number of sodium and potassium in the two structures. Whereas sodium has a fourfold coordination in NaCuIn(PO₄)₂, potassium is surrounded by nine oxygen atoms in KCuFe(PO₄)₂ because of its greater ionic radius.

Bond-valence-sum calculations (Brown & Altermatt, 1985 ) are in good agreement with the expected values (in valence units) for sodium(I), copper(II), indium(III) and the phosphorus(V) cations, viz. Na^I = 0.845 (2), Cu^II = 2.102 (3), In^III = 3.152 (4), P1^V = 4.930 (8), and P2^V = 4.992 (8). For the oxygen anions, the calculated values range between 1.940 (5) and 2.076 (3).

3. Database survey

Phosphate-based materials with general formula AM^IIM′^III(PO₄)₂ commonly show crystal structures where channels or, more rarely, layers are formed by the [M^IIM′^II(PO₄)₂]⁻ framework to delimit suitable environments to accommodate the A⁺ cations. A recent survey given by Yakubovich et al. (2019 ) revealed that all compounds of the morphotropic series AM^IIM′^III(PO₄)₂, where A = Na, K, Rb or NH₄, M′′ = Cu, Ni, Co, Fe, Zn or Mg and M′′′ = Fe, Al or Ga, crystallize in the monoclinic crystal system and can be classified into seven subgroups according to their structure types, viz. (i) KNiFe(PO₄)₂ (space-group type P2₁/c, Z = 4; Strutynska et al., 2014 ); (ii) KFe^IIFe^III(PO₄)₂ (space-group type P2₁/c, Z = 4; Yakubovich et al., 1986 ); (iii) (NH₄)Fe^IIFe^III(PO₄)₂ (space-group type C2/c, Z =16; Boudin & Lii, 1998 ); (iv) K(Co,Al)₂(PO₄)₂ (space-group type C2/c, Z = 8; Chen et al., 1997 ); (v) (NH₄)(Zn,Ga)₂(PO₄)₂ (space-group type P2₁/a, Z = 4; Logar et al., 2001 ); (vi) KMgFe(PO₄)₂ (space-group type C2/c, Z = 4; Badri et al., 2009 ); (vii) NaZnAl(PO₄)₂ (space-group type P2₁/c, Z = 4; Yakubovich et al., 2019). NaCuIn(PO₄)₂ belongs to the second subgroup of this classification.

In addition, the structures of certain members of this phosphate family are similar to those of the zeolite-ABW structural type (Badri et al., 2014 ). When the trivalent cation is lanthanum or yttrium, the crystal structures KM^IILa(PO₄)₂ (M^II = Mg or Zn) are isotypes of the monazite monoclinic structure of LaPO₄ with space-group type P2₁/n (Pan et al., 2006; Tie et al., 1995), while KMgY(PO₄)₂ turns out to be an isotype of the xenotime structure YPO₄ adopting a tetragonal symmetry with space-group type I4₁/amd (Tie et al., 1996 ).

4. Synthesis and crystallization

Stoichiometric amounts of NaNO₃, CuO, In₂O₃ and NH₄H₂PO₄ as precursors in the molar ratio 1:1:0.5:2 were ground in an agate mortar and pre-heated at 473 and 673 K in a platinum crucible to eliminate gaseous products. The resulting powder was subsequently heated to a temperature of 1473 K. The product was then cooled to room temperature at a rate of 5 K h⁻¹. The obtained product contained green single crystals corresponding to the title phosphate.

5. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 1.

Table 1
Experimental details

Crystal data
Chemical formula	NaCuIn(PO₄)₂
M_r	391.29
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	296
a, b, c (Å)	8.2563 (3), 10.1382 (4), 8.8060 (3)
β (°)	114.444 (1)
V (Å³)	671.03 (4)
Z	4
Radiation type	Mo Kα
μ (mm⁻¹)	7.16
Crystal size (mm)	0.34 × 0.25 × 0.19

Data collection
Diffractometer	Bruker X8 APEX Diffractometer
Absorption correction	Multi-scan (SADABS; Krause et al., 2015 )
T_min, T_max	0.528, 0.747
No. of measured, independent and observed [I > 2σ(I)] reflections	24292, 3106, 2996
R_int	0.026
(sin θ/λ)_max (Å⁻¹)	0.820

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.013, 0.033, 1.11
No. of reflections	3106
No. of parameters	119
Δρ_max, Δρ_min (e Å⁻³)	0.66, −0.59
Computer programs: APEX2 and SAINT (Bruker, 2009 ), SHELXT2014/5 (Sheldrick, 2015a ), SHELXL2018/3 (Sheldrick, 2015b ), ORTEP-3 for Windows (Farrugia, 2012 ), DIAMOND (Brandenburg, 2006 ) and publCIF (Westrip, 2010 ).

Labelling of atoms and their coordinates were adapted from isotypic KCuFe(PO₄)₂ (Badri et al., 2011). Since not all atoms in the latter description are part of one unit cell, a translation by (z + 1) relative to the original coordinates brings all corresponding atoms inside one unit cell. Moreover, oxygen atoms O11 and O14 were translated by (x − $[{1\over 2}]$ , −y + $[{1\over 2}]$ , z − $[{1\over 2}]$ ) and (x, y, z − 1), respectively, to be linked directly to P1.

The maximum and minimum electron densities in the final difference-Fourier map are at 0.70 Å from O14 and 0.50 Å from Cu1, respectively.

Supporting information

CCDC reference: 1983244

Crystal structure: contains datablock I. DOI: https://doi.org/10.1107/S2056989020001929/wm5539sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2056989020001929/wm5539Isup2.hkl

checkCIF report

Computing details top

Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SHELXT2014/5 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2015b); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012), DIAMOND (Brandenburg, 2006); software used to prepare material for publication: publCIF (Westrip, 2010).

Sodium copper(II) indium bis[phosphate(V)] top

Crystal data top

NaCuIn(PO₄)₂	F(000) = 732
M_r = 391.29	D_x = 3.873 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
a = 8.2563 (3) Å	Cell parameters from 3106 reflections
b = 10.1382 (4) Å	θ = 2.9–35.6°
c = 8.8060 (3) Å	µ = 7.16 mm⁻¹
β = 114.444 (1)°	T = 296 K
V = 671.03 (4) Å³	Block, green
Z = 4	0.34 × 0.25 × 0.19 mm

Data collection top

Bruker X8 APEX Diffractometer	3106 independent reflections
Radiation source: fine-focus sealed tube	2996 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.026
φ and ω scans	θ_max = 35.6°, θ_min = 2.9°
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	h = −12→13
T_min = 0.528, T_max = 0.747	k = −16→16
24292 measured reflections	l = −14→14

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.0139P)² + 0.5758P] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.013	(Δ/σ)_max = 0.004
wR(F²) = 0.033	Δρ_max = 0.66 e Å⁻³
S = 1.11	Δρ_min = −0.59 e Å⁻³
3106 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick, 2015b), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
119 parameters	Extinction coefficient: 0.0093 (3)

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Na1	0.51418 (10)	−0.16856 (7)	1.09748 (8)	0.01965 (13)
Cu1	0.37225 (2)	0.11940 (2)	0.45881 (2)	0.00706 (3)
In1	0.00214 (2)	0.12812 (2)	0.73403 (2)	0.00463 (3)
P1	0.12997 (4)	0.17027 (3)	0.15664 (4)	0.00494 (5)
O11	−0.03216 (13)	0.25215 (10)	0.13588 (12)	0.01037 (15)
O12	0.30223 (12)	0.24790 (9)	0.27141 (11)	0.00812 (14)
O13	0.14612 (12)	0.04925 (9)	0.27222 (11)	0.00824 (14)
O14	0.13759 (14)	0.12965 (10)	−0.00448 (12)	0.01159 (16)
P2	0.28460 (4)	−0.08358 (3)	0.66933 (4)	0.00448 (5)
O21	0.11495 (13)	−0.13653 (9)	0.52826 (12)	0.00993 (15)
O22	0.37706 (12)	−0.19241 (8)	0.79630 (11)	0.00787 (14)
O23	0.24068 (13)	0.03111 (9)	0.75876 (12)	0.00903 (15)
O24	0.41607 (13)	−0.03247 (9)	0.59836 (12)	0.00962 (15)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Na1	0.0288 (3)	0.0145 (3)	0.0146 (3)	−0.0042 (2)	0.0079 (3)	−0.0035 (2)
Cu1	0.00887 (7)	0.00557 (6)	0.00492 (6)	−0.00104 (4)	0.00104 (5)	0.00126 (4)
In1	0.00517 (4)	0.00405 (4)	0.00432 (4)	−0.00022 (2)	0.00161 (3)	−0.00042 (2)
P1	0.00552 (11)	0.00490 (11)	0.00367 (11)	−0.00020 (9)	0.00119 (9)	0.00053 (8)
O11	0.0096 (4)	0.0125 (4)	0.0094 (4)	0.0054 (3)	0.0044 (3)	0.0042 (3)
O12	0.0085 (4)	0.0077 (3)	0.0063 (3)	−0.0034 (3)	0.0012 (3)	0.0008 (3)
O13	0.0091 (4)	0.0055 (3)	0.0071 (3)	−0.0028 (3)	0.0004 (3)	0.0020 (3)
O14	0.0129 (4)	0.0165 (4)	0.0043 (3)	0.0025 (3)	0.0025 (3)	−0.0014 (3)
P2	0.00536 (11)	0.00392 (11)	0.00410 (11)	0.00089 (8)	0.00189 (9)	0.00025 (8)
O21	0.0096 (4)	0.0119 (4)	0.0054 (3)	−0.0026 (3)	0.0002 (3)	−0.0013 (3)
O22	0.0109 (4)	0.0058 (3)	0.0073 (3)	0.0032 (3)	0.0041 (3)	0.0027 (3)
O23	0.0088 (4)	0.0071 (3)	0.0113 (4)	0.0018 (3)	0.0042 (3)	−0.0034 (3)
O24	0.0101 (4)	0.0092 (4)	0.0125 (4)	0.0030 (3)	0.0077 (3)	0.0056 (3)

Geometric parameters (Å, º) top

Na1—O21ⁱ	2.3213 (12)	In1—O22^viii	2.1441 (9)
Na1—O23ⁱⁱ	2.3496 (12)	In1—O13^vii	2.1632 (9)
Na1—O22	2.4268 (11)	In1—O12^ix	2.2051 (9)
Na1—O11ⁱⁱⁱ	2.4275 (11)	P1—O14	1.5035 (10)
Cu1—O24	1.9088 (9)	P1—O11	1.5205 (10)
Cu1—O11^iv	1.9317 (9)	P1—O13	1.5642 (9)
Cu1—O12	1.9913 (9)	P1—O12	1.5729 (9)
Cu1—O13	2.0378 (9)	P2—O23	1.5297 (9)
Cu1—O24^v	2.1939 (9)	P2—O22	1.5310 (9)
In1—O14^vi	2.1028 (10)	P2—O21	1.5340 (10)
In1—O21^vii	2.1044 (9)	P2—O24	1.5488 (9)
In1—O23	2.1303 (9)

O21ⁱ—Na1—O23ⁱⁱ	108.90 (4)	O14^vi—In1—O13^vii	94.18 (4)
O21ⁱ—Na1—O22	71.58 (4)	O21^vii—In1—O13^vii	90.44 (4)
O23ⁱⁱ—Na1—O22	123.80 (4)	O23—In1—O13^vii	96.21 (4)
O21ⁱ—Na1—O11ⁱⁱⁱ	94.99 (4)	O22^viii—In1—O13^vii	171.80 (3)
O23ⁱⁱ—Na1—O11ⁱⁱⁱ	88.91 (4)	O14^vi—In1—O12^ix	85.65 (4)
O22—Na1—O11ⁱⁱⁱ	146.95 (4)	O21^vii—In1—O12^ix	96.23 (4)
O24—Cu1—O11^iv	96.82 (4)	O23—In1—O12^ix	164.87 (3)
O24—Cu1—O12	166.88 (4)	O22^viii—In1—O12^ix	87.16 (3)
O11^iv—Cu1—O12	96.28 (4)	O13^vii—In1—O12^ix	91.55 (3)
O24—Cu1—O13	95.96 (4)	O14—P1—O11	114.50 (6)
O11^iv—Cu1—O13	144.90 (4)	O14—P1—O13	111.94 (5)
O12—Cu1—O13	72.85 (3)	O11—P1—O13	109.89 (5)
O24—Cu1—O24^v	82.35 (4)	O14—P1—O12	111.32 (5)
O11^iv—Cu1—O24^v	110.97 (4)	O11—P1—O12	108.72 (5)
O12—Cu1—O24^v	93.34 (4)	O13—P1—O12	99.40 (5)
O13—Cu1—O24^v	103.05 (4)	O23—P2—O22	108.94 (5)
O14^vi—In1—O21^vii	174.97 (4)	O23—P2—O21	110.57 (5)
O14^vi—In1—O23	80.87 (4)	O22—P2—O21	110.58 (5)
O21^vii—In1—O23	96.68 (4)	O23—P2—O24	107.97 (5)
O14^vi—In1—O22^viii	93.79 (4)	O22—P2—O24	108.36 (5)
O21^vii—In1—O22^viii	81.66 (3)	O21—P2—O24	110.35 (5)
O23—In1—O22^viii	86.94 (4)

Symmetry codes: (i) x+1/2, −y−1/2, z+1/2; (ii) −x+1, −y, −z+2; (iii) −x+1/2, y−1/2, −z+3/2; (iv) x+1/2, −y+1/2, z+1/2; (v) −x+1, −y, −z+1; (vi) x, y, z+1; (vii) −x, −y, −z+1; (viii) −x+1/2, y+1/2, −z+3/2; (ix) x−1/2, −y+1/2, z+1/2.

Acknowledgements

The authors thank the Unit of Support for Technical and Scientific Research (UATRS, CNRST) for the X-ray measurements.

Funding information

Mohammed V University, Rabat, Morocco, is thanked for financial support.

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